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Method for preparing amino modified mesoporous silicon dioxide for separating and purifying paclitaxel

A technology of mesoporous silica and amino modification, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of poor purification effect and low yield of paclitaxel, and achieve Good selection of adsorption performance, high yield, and low cost of raw materials

Inactive Publication Date: 2017-07-14
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the technical defects of the prior art, and provides a preparation method of amino-modified mesoporous silica for the separation and purification of paclitaxel, so as to solve the problem of poor purification effect and low yield of paclitaxel in the prior art. technical problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] ① Take 10g of spherical silica (20 mesh) and add it to 10mL of Piranha solution (hydrogen peroxide: concentrated sulfuric acid = 3 / 7, v / v), stir with a rotor, and put it in an oil bath at 120°C for 60min. Cool to room temperature, dilute the Piranha solution with ethanol (concentrated sulfuric acid may exotherm at this time), filter after cooling, and wash with ethanol repeatedly 5 times until neutral. Vacuum-dry at 60°C for 12 hours to obtain activated silica, which is ready for use.

[0033] ②Under nitrogen atmosphere, 1.5 mL of functionalization reagent (3-aminopropyl-triethoxysilane) was dissolved in 10 mL of absolute ethanol, and the mixed solution was stirred at 50° C. for 1 h. 0.1 g of surfactant Pluronic F127, 1.0 g of activated silicon dioxide, and 0.5 mL of tetraethyl orthosilicate (TEOS) were added to the system. Add 3.0 mL of 1 mol / L catalyst HCl dropwise, keep stirring at 50°C for 1 h under a nitrogen atmosphere, and then keep 50°C and incubate on a shakin...

Embodiment 2

[0037]① Take 10g of spherical silica (300 mesh) and add it to 10mL of Piranha solution (hydrogen peroxide: concentrated sulfuric acid = 3 / 7, v / v), stir with a rotor, and put it in an oil bath at 120°C for 60min. Cool to room temperature, dilute the Piranha solution with ethanol (concentrated sulfuric acid may exotherm at this time), filter after cooling, and wash with ethanol repeatedly 10 times until neutral. Vacuum-dry at 60°C for 12 hours to obtain activated silica, which is ready for use.

[0038] ②Under a nitrogen atmosphere, 3.5 mL of the functionalization reagent 3-aminopropyl-triethoxysilane was dissolved in 50 mL of absolute ethanol, and the mixed solution was stirred at 50°C for 6 hours. 0.59 surfactant CTAB, 1.0 g of activated silicon dioxide, and 2.5 mL of tetraethyl orthosilicate (TEOS) were added to the system. 1mol / L catalyst NH 4 7.0 mL of OH was added dropwise, kept at 50°C and stirred for 2h under nitrogen atmosphere, then kept at 50°C and incubated on a sh...

Embodiment 3

[0042] ① Take 10g of spherical silica (200 mesh) and add it to 50mL of Piranha solution (hydrogen peroxide: concentrated sulfuric acid = 3 / 7, v / v), stir with a rotor, and put it in an oil bath at 120°C for 60min. Cool to room temperature, dilute the Piranha solution with ethanol (concentrated sulfuric acid may be exothermic at this time), filter after cooling, and rinse repeatedly with ethanol 8 times until neutral. Vacuum-dry at 60°C for 12 hours to obtain activated silica, which is ready for use.

[0043] ②Under a nitrogen atmosphere, dissolve 2.5 mL of the functionalization reagent N-aminoethyl-γ-aminopropyltrimethoxysilane in 50 mL of absolute ethanol, and stir the mixed solution at 50°C for 6 hours. 0.5g of surfactant PluronicF127, 1.0g of activated silicon dioxide, and 1.0mL of tetraethyl orthosilicate (TEOS) were added to the system. 5.0 mL of 1 mol / L catalyst HCl was added dropwise, kept at 50°C and stirred for 2 hours under nitrogen atmosphere, and then kept at 50°C ...

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Abstract

The invention provides a method for preparing amino modified mesoporous silicon dioxide for separating and purifying paclitaxel. According to the method, the amino modified mesoporous silicon dioxide is prepared on the surface of spherical silicon dioxide with the particle size of 20 to 300 meshes, which serves as a support, through taking amino containing silane as a functionalization reagent and taking a surfactant as a soft template agent, and the product can be used for separating and purifying the paclitaxel as a chromatographic filler. The amino modified mesoporous silicon dioxide material prepared by the method presents good selective adsorption performance to the paclitaxel; and through column chromatography, the yield of the paclitaxel in an extract sample can be greatly increased. The amino modified mesoporous silicon dioxide material prepared by the method is low in raw material cost, and the preparation process and a process for separating the target object are simple in operation and high in yield, so that large-scale application in industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of separation of natural medicines, and further relates to the preparation technology of chromatography packing, in particular to a preparation method of amino-modified mesoporous silica for separating and purifying paclitaxel. Background technique [0002] Paclitaxel is a diterpenoid compound originally extracted from the bark of Taxus brevifolia by American chemist Wani et al. in 1971. In 1979, Horwitz and others in the United States first discovered that it has good anticancer activity and unique effects of inhibiting microtubule depolymerization and stabilizing microtubules. It can be used for first-line and second-line treatment of ovarian cancer, breast cancer and non-small cell lung cancer. Neck cancer, esophageal cancer, seminoma, relapsed non-Hodgkin's lymphoma, etc. also have definite therapeutic activity. With the continuous deepening of clinical research, paclitaxel was approved by the US FDA in...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/28B01J20/30B01D15/08C07D305/14
CPCB01J20/103B01D15/08B01J20/28019B01J20/28083C07D305/14
Inventor 范杰平袁天桃许小康
Owner NANCHANG UNIV
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